反应详情

温度

45 °C

A solution of tert-butyl 4-cyclopropylpiperazine-1-carboxylate (92 g) in 1,4-dioxin (200 mL) was treated with HCl (4 M in 1,4-dioxin, 500 mL) over 10 min while maintaining the temperature below 40° C. After the addition was complete, the mixture was heated at 45° C. for 9 h and then was cooled to room temperature. The thick suspension was diluted with hexanes (400 mL) and was cooled to 10° C. The resulting solid was collected by filtration, washed with hexanes, and dried to yield the title compound as a white solid.

1. temperaturewhile maintaining the temperature below 40° C
2. additionAfter the addition
3. temperaturewas cooled to room temperature
4. temperaturewas cooled to 10° C
5. filtrationThe resulting solid was collected by filtration
6. washwashed with hexanes
7. customdried